High-pressure bulk synthesis of crystalline C6N9H3·HCl

A novel C3N4 graphitic derivative

Z. Zhang, Kurt Leinenweber, M. Bauer, Laurence Garvie, P. F. McMillan, George Wolf

Research output: Contribution to journalArticle

185 Citations (Scopus)

Abstract

A novel carbon nitride compound, structurally related to the proposed graphitic phase of C3N4, has been synthesized in a bulk well-crystallized form. The new material, with stoichiometry C6N9H4Cl, was prepared through a solid-state reaction of 2,4,6-triamino-1,3,5-triazine with 2,4,6-trichloro-1,3,5-triazine at 1.0-1.5 GPa and 500-550 °C and also through a self-reaction of 2-amino-4,6-dichloro-1,3,5-triazine at similar conditions. X-ray and electron diffraction measurements on the yellowish compound indicate a hexagonal space group (P63/m) with cell parameters of a = 8.4379(10) Å and c = 6.4296(2) Å. This new compound possesses a two-dimensional C6N9H3 framework that is structurally related to the hypothetical P6m2 graphitic phase of C3N4, but with an ordered arrangement of C3N3 voids. The large voids in the graphene sheets are occupied by chloride ions with an equivalent number of nitrogen atoms on the framework protonated for charge balance. The composition of the sample was determined by bulk chemical analysis and confirmed by electron energy loss (EELS) spectroscopy. The chemical and structural model is consistent with bulk density measurements and with the infrared and 13C NMR spectra. This work represents the first bulk synthesis of a well-characterized and highly crystalline material containing a continuous network of alternating carbon and nitrogen atoms.

Original languageEnglish (US)
Pages (from-to)7788-7796
Number of pages9
JournalJournal of the American Chemical Society
Volume123
Issue number32
DOIs
StatePublished - 2001

Fingerprint

Triazines
Electron Energy-Loss Spectroscopy
Nitrogen
Crystalline materials
Chemical Models
Derivatives
Pressure
Atoms
Graphite
Carbon nitride
Electron energy loss spectroscopy
Structural Models
Chemical analysis
Solid state reactions
Electron diffraction
X-Ray Diffraction
Stoichiometry
Graphene
Chlorides
Carbon

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

High-pressure bulk synthesis of crystalline C6N9H3·HCl : A novel C3N4 graphitic derivative. / Zhang, Z.; Leinenweber, Kurt; Bauer, M.; Garvie, Laurence; McMillan, P. F.; Wolf, George.

In: Journal of the American Chemical Society, Vol. 123, No. 32, 2001, p. 7788-7796.

Research output: Contribution to journalArticle

@article{4d575f9b6a884e709c3b8a9343d979bd,
title = "High-pressure bulk synthesis of crystalline C6N9H3·HCl: A novel C3N4 graphitic derivative",
abstract = "A novel carbon nitride compound, structurally related to the proposed graphitic phase of C3N4, has been synthesized in a bulk well-crystallized form. The new material, with stoichiometry C6N9H4Cl, was prepared through a solid-state reaction of 2,4,6-triamino-1,3,5-triazine with 2,4,6-trichloro-1,3,5-triazine at 1.0-1.5 GPa and 500-550 °C and also through a self-reaction of 2-amino-4,6-dichloro-1,3,5-triazine at similar conditions. X-ray and electron diffraction measurements on the yellowish compound indicate a hexagonal space group (P63/m) with cell parameters of a = 8.4379(10) {\AA} and c = 6.4296(2) {\AA}. This new compound possesses a two-dimensional C6N9H3 framework that is structurally related to the hypothetical P6m2 graphitic phase of C3N4, but with an ordered arrangement of C3N3 voids. The large voids in the graphene sheets are occupied by chloride ions with an equivalent number of nitrogen atoms on the framework protonated for charge balance. The composition of the sample was determined by bulk chemical analysis and confirmed by electron energy loss (EELS) spectroscopy. The chemical and structural model is consistent with bulk density measurements and with the infrared and 13C NMR spectra. This work represents the first bulk synthesis of a well-characterized and highly crystalline material containing a continuous network of alternating carbon and nitrogen atoms.",
author = "Z. Zhang and Kurt Leinenweber and M. Bauer and Laurence Garvie and McMillan, {P. F.} and George Wolf",
year = "2001",
doi = "10.1021/ja0103849",
language = "English (US)",
volume = "123",
pages = "7788--7796",
journal = "Journal of the American Chemical Society",
issn = "0002-7863",
publisher = "American Chemical Society",
number = "32",

}

TY - JOUR

T1 - High-pressure bulk synthesis of crystalline C6N9H3·HCl

T2 - A novel C3N4 graphitic derivative

AU - Zhang, Z.

AU - Leinenweber, Kurt

AU - Bauer, M.

AU - Garvie, Laurence

AU - McMillan, P. F.

AU - Wolf, George

PY - 2001

Y1 - 2001

N2 - A novel carbon nitride compound, structurally related to the proposed graphitic phase of C3N4, has been synthesized in a bulk well-crystallized form. The new material, with stoichiometry C6N9H4Cl, was prepared through a solid-state reaction of 2,4,6-triamino-1,3,5-triazine with 2,4,6-trichloro-1,3,5-triazine at 1.0-1.5 GPa and 500-550 °C and also through a self-reaction of 2-amino-4,6-dichloro-1,3,5-triazine at similar conditions. X-ray and electron diffraction measurements on the yellowish compound indicate a hexagonal space group (P63/m) with cell parameters of a = 8.4379(10) Å and c = 6.4296(2) Å. This new compound possesses a two-dimensional C6N9H3 framework that is structurally related to the hypothetical P6m2 graphitic phase of C3N4, but with an ordered arrangement of C3N3 voids. The large voids in the graphene sheets are occupied by chloride ions with an equivalent number of nitrogen atoms on the framework protonated for charge balance. The composition of the sample was determined by bulk chemical analysis and confirmed by electron energy loss (EELS) spectroscopy. The chemical and structural model is consistent with bulk density measurements and with the infrared and 13C NMR spectra. This work represents the first bulk synthesis of a well-characterized and highly crystalline material containing a continuous network of alternating carbon and nitrogen atoms.

AB - A novel carbon nitride compound, structurally related to the proposed graphitic phase of C3N4, has been synthesized in a bulk well-crystallized form. The new material, with stoichiometry C6N9H4Cl, was prepared through a solid-state reaction of 2,4,6-triamino-1,3,5-triazine with 2,4,6-trichloro-1,3,5-triazine at 1.0-1.5 GPa and 500-550 °C and also through a self-reaction of 2-amino-4,6-dichloro-1,3,5-triazine at similar conditions. X-ray and electron diffraction measurements on the yellowish compound indicate a hexagonal space group (P63/m) with cell parameters of a = 8.4379(10) Å and c = 6.4296(2) Å. This new compound possesses a two-dimensional C6N9H3 framework that is structurally related to the hypothetical P6m2 graphitic phase of C3N4, but with an ordered arrangement of C3N3 voids. The large voids in the graphene sheets are occupied by chloride ions with an equivalent number of nitrogen atoms on the framework protonated for charge balance. The composition of the sample was determined by bulk chemical analysis and confirmed by electron energy loss (EELS) spectroscopy. The chemical and structural model is consistent with bulk density measurements and with the infrared and 13C NMR spectra. This work represents the first bulk synthesis of a well-characterized and highly crystalline material containing a continuous network of alternating carbon and nitrogen atoms.

UR - http://www.scopus.com/inward/record.url?scp=0034808010&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0034808010&partnerID=8YFLogxK

U2 - 10.1021/ja0103849

DO - 10.1021/ja0103849

M3 - Article

VL - 123

SP - 7788

EP - 7796

JO - Journal of the American Chemical Society

JF - Journal of the American Chemical Society

SN - 0002-7863

IS - 32

ER -